The feasibility of Fourier transform-infrared (FT-IR) spectroscopy for determining the monosaccharide composition of glycoconjugates is being tested. This technique is being considered as a stand-alone method for glycosyl composition analysis and as an adjunct to capillary electrophoretic (CE) separation of the monosaccharide components of glycoconjugates. Results indicate that FT-IR spectroscopy can be used to differentiate among a wide spectrum of monosaccharide isomers, and that buffers typically used for CE separations do not interfere with IR detection. Additionally, FT-IR spectroscopy appears to have potential for determining the monosaccharide composition of glycoprotein oligosaccharides without the need for derivatization, separation, or hydrolysis.